CN108059189B - Preparation method of molybdenum disulfide nanotube - Google Patents
Preparation method of molybdenum disulfide nanotube Download PDFInfo
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Abstract
The invention discloses a preparation method of a molybdenum disulfide nanotube, which comprises the following process steps: 1) paving molybdenum hexacarbonyl at the bottom of a ceramic crucible, then placing a porous anodic aluminum oxide template with an opening downward above the molybdenum hexacarbonyl, sealing the crucible, placing the crucible in a tubular furnace, carrying out low-temperature sublimation deposition and high-temperature pyrolysis under the protection of gas, and then cooling; 2) after the temperature of the vacuum tube furnace is reduced to room temperature, the opening of the template is downwards placed in a ceramic crucible filled with sulfur powder, the crucible is sealed, and then the temperature is raised under the protection of gas, so that elemental sulfur and metal molybdenum directly react; 3) removing the porous alumina template by using a dilute acid solution, removing redundant sulfur by using carbon disulfide, then carrying out suction filtration treatment, and drying to obtain a finished product. The method has simple steps, no environmental pollution and no need of complex equipment, and the prepared molybdenum disulfide nanotube powder material has strong size controllability, good crystallinity and uniform nanotube wall morphology, thereby greatly improving the comprehensive performance of the finished product of the molybdenum disulfide nanotube powder material. The invention has wide applicability and is beneficial to large-scale industrial production.
Description
Technical Field
The invention relates to the field of semiconductor nano materials, in particular to a preparation method of a semiconductor nano tube.
Background
Molybdenum disulfide (MoS)2) The crystal has a layered close-packed hexagonal structure, the crystal is combined in the layer through a stronger covalent bond, weak van der waals force is formed between the layers, the crystal is easy to slide along a close-packed surface, the crystal has good anisotropy and lower friction coefficient, and sulfur element exposed on the surface of the crystal generates strong adhesion to metal to form a firm film, so that molybdenum disulfide can be well attached to the surface of the metal to play a lubricating function all the time, the lubricating property is superior to that of graphite, and particularly, the crystal still has lower friction coefficient under the conditions of high temperature, high vacuum and the like. It has diamagnetic property, can be used as a linear photoconductor and a semiconductor for displaying P-type or N-type conductivity, and has rectifying and transducing functions. Molybdenum disulfide is also useful as a catalyst for the dehydrogenation of complex hydrocarbons. The molybdenum disulfide crystal is a direct band gap semiconductor, and the forbidden band width of the molybdenum disulfide crystal is about 1.9eV and is far larger than that of a silicon material (1.12 eV). Due to the wide forbidden band property of the molybdenum disulfide, the defects of zero band gap and BN wide band gap of graphene are overcome, so that the molybdenum disulfide has very obvious application in logic devices with high on-off ratio and low power consumption. Compared with silicon materials, molybdenum disulfide is a direct bandgap semiconductor, meaning that photons can be efficiently absorbed or emitted through bandgap transitions, and also offers the possibility of application in the field of optoelectronic devices. The characteristics of the molybdenum disulfide, such as wide forbidden band, no dangling bond and the like, are considered to be a potential material in the post-silicon era. Theoretical simulation shows that the performance parameters of the molybdenum disulfide electronic device can meet the requirements of the international semiconductor technologyThe performance index of logic devices in 2023, which is presented by the diagram (ITRS), is therefore of great interest.
As early as 1992, the Tenne research and development team discovered WS with a Fullerene structure2Nanoparticles and nanotubes, followed by synthesis of MoS using a similar method2Nanoparticles and nanotubes. From this MoS2The preparation and research work of nano materials is continuously carried out. C, N, R, Rao et al direct pyrolysis of (NH) in hydrogen at 1200-1300 deg.C4)2MoS4And (NH)4)2WS4MoS is obtained2And WS2A nanotube. In 2011, Zhuyanfang et al thermally decomposed ammonium tetrathiomolybdate precursor in alumina template to prepare molybdenum disulfide nanotubes. Chinese patent' C/MoS2Method for preparing composite material, product and electrochemical application thereof (application number: 201510692438.5), wherein MoS is prepared by hydrothermal reaction of ammonium molybdate and sulfur2A nanotube. However, the above-mentioned prior reports have been made in the preparation of MoS2The nanotube process involves complex chemical reaction, the operation difficulty is large, the size of the obtained molybdenum sulfide nanotube is uncontrollable, and great influence is brought to the electronic application of the molybdenum sulfide nanotube.
Disclosure of Invention
The invention aims to provide a preparation method of a molybdenum disulfide nanotube aiming at the defects of the prior art, and the obtained molybdenum disulfide nanotube powder material has wide applicability and excellent comprehensive performance and can be applied to electronic devices.
The technical scheme adopted by the invention is as follows: a preparation method of a molybdenum disulfide nanotube comprises the following process steps:
1) taking molybdenum hexacarbonyl as a raw material and porous anodic aluminum oxide as a template, paving the raw material at the bottom of a ceramic crucible, then placing the porous anodic aluminum oxide template with an opening downward above the raw material, sealing the crucible, placing the crucible in a vacuum tube furnace, heating under the protection of gas, sublimating at low temperature to deposit the molybdenum hexacarbonyl in the porous anodic aluminum oxide template, continuously heating to deposit the molybdenum hexacarbonyl in the porous anodic aluminum oxide template for thermal decomposition to obtain metal molybdenum deposit;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with sulfur powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating under the protection of gas to enable elemental sulfur to directly react with metal molybdenum, stopping heating after the reaction is finished, and cooling the crucible to the room temperature along with the furnace;
3) removing the porous alumina template by using a dilute acid solution, removing redundant sulfur by using carbon disulfide, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain a finished product.
As a further improvement of the scheme, the pore diameter of the porous anodic alumina template in the step 1) is within the range of 10-200 nm. In particular, the shape controllability of the nanotube can be stronger by limiting the pore diameter of the porous anodic alumina template.
As a further improvement of the scheme, the low-temperature sublimation temperature in the step 1) is 50-150 ℃, and the sublimation time is 30-200 min. The invention directly obtains the deposit through low-temperature sublimation, and the limit of the sublimation temperature and the heat preservation time can ensure that the molybdenum hexacarbonyl is more fully deposited.
As a further improvement of the scheme, the thermal decomposition temperature in the step 1) is 200-420 ℃, and the thermal decomposition time is 30-100 min. In particular, the limitation of the pyrolysis temperature and the pyrolysis time can effectively improve the crystallinity of the metal molybdenum in the alumina template.
As a further improvement of the scheme, in the step 2), the reaction temperature of the elemental sulfur and the metal molybdenum is 500-650 ℃, and the reaction time is 100-150 min. In particular, the reaction temperature and the reaction time of the molybdenum disulfide are limited so that the reaction is more complete.
As a further improvement of the scheme, the dilute acid solution in the step 3) is a phosphoric acid solution with the concentration of 0.1-3 mol/L. In particular, further definition of dilute acid solution allows for more efficient removal of the alumina template.
As a further improvement of the scheme, the gas in the step 1) and the step 2) is nitrogen or argon, the gas purity is 99.999%, and the flow rate of the protective gas is 10-500 SCCM.
The invention has the beneficial effects that: the method has simple steps, realizes the direct reaction of the molybdenum metal and the sulfur powder in the limited space to prepare the molybdenum disulfide nanotube powder material, has no environmental pollution, does not need complex equipment, and has strong size controllability, good crystallinity and uniform nanotube wall appearance of the prepared molybdenum disulfide nanotube powder material, thereby greatly improving the comprehensive performance of the finished product of the molybdenum disulfide nanotube powder material. The invention has wide applicability and is beneficial to large-scale industrial production.
Detailed Description
The present invention is specifically described below with reference to examples in order to facilitate understanding of the present invention by those skilled in the art. It should be particularly noted that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as non-essential improvements and modifications to the invention may occur to those skilled in the art, which fall within the scope of the invention as defined by the appended claims. Meanwhile, the raw materials mentioned below are not specified in detail and are all commercial products; the process steps or preparation methods not mentioned in detail are all process steps or preparation methods known to the person skilled in the art.
Example 1
A preparation method of a molybdenum disulfide nanotube comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM nitrogen to clean air in the furnace tube. Under the protection of 100SCCM nitrogen, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with sulfur powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 120 ℃ under the protection of 100SCCM nitrogen, keeping the temperature for 1h, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out the sample, removing the porous alumina template by using a phosphoric acid solution with the concentration of 0.3mol/L, removing redundant sulfur powder by using carbon disulfide, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum disulfide nanotube powder material in the embodiment 1.
Example 2
A preparation method of a molybdenum disulfide nanotube comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 10nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM nitrogen to clean air in the furnace tube. Under the protection of 100SCCM nitrogen, heating to 50 ℃ and preserving heat for 200min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with sulfur powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 120 ℃ under the protection of 100SCCM nitrogen gas, keeping the temperature for 60min, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out the sample, removing the porous alumina template by using a phosphoric acid solution with the concentration of 0.3mol/L, removing redundant sulfur powder by using carbon disulfide, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain a finished product of the molybdenum disulfide nanotube powder material in the embodiment 2.
Example 3
A preparation method of a molybdenum disulfide nanotube comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM nitrogen to clean air in the furnace tube. Under the protection of 100SCCM nitrogen, heating to 150 ℃ and preserving heat for 30min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with sulfur powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 120 ℃ under the protection of 100SCCM nitrogen, keeping the temperature for 1h, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out the sample, removing the porous alumina template by using a phosphoric acid solution with the concentration of 0.3mol/L, removing redundant sulfur powder by using carbon disulfide, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain a finished product of the molybdenum disulfide nanotube powder material in the embodiment 3.
Example 4
A preparation method of a molybdenum disulfide nanotube comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 200nm with an opening facing downwards above the molybdenum hexacarbonyl, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM nitrogen to clean air in the furnace tube. Under the protection of 100SCCM nitrogen, heating to 100 ℃ and preserving heat for 1h, then continuing heating to 200 ℃ and preserving heat for 100min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with sulfur powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 120 ℃ under the protection of 100SCCM nitrogen gas, keeping the temperature for 60min, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out the sample, removing the porous alumina template by using a phosphoric acid solution with the concentration of 0.3mol/L, removing redundant sulfur powder by using carbon disulfide, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum disulfide nanotube powder material in the embodiment 4.
Example 5
A preparation method of a molybdenum disulfide nanotube comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 100SCCM nitrogen to clean air in the furnace tube. Under the protection of 100SCCM nitrogen, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 420 ℃ and preserving heat for 30min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with sulfur powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 120 ℃ under the protection of 100SCCM nitrogen gas, keeping the temperature for 60min, continuing heating to 550 ℃ and keeping the temperature for 120min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out the sample, removing the porous alumina template by using a phosphoric acid solution with the concentration of 0.1mol/L, removing redundant sulfur powder by using carbon disulfide, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum disulfide nanotube powder material in the embodiment 5.
Example 6
A preparation method of a molybdenum disulfide nanotube comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 500SCCM argon to clean air in the furnace tube. Under the protection of argon gas of 500SCCM, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with sulfur powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 110 ℃ under the protection of 500SCCM argon gas, keeping the temperature for 120min, continuing heating to 500 ℃ and keeping the temperature for 150min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out the sample, removing the porous alumina template by using a phosphoric acid solution with the concentration of 0.3mol/L, removing redundant sulfur powder by using carbon disulfide, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain the finished product of the molybdenum disulfide nanotube powder material in the embodiment 6.
Example 7
A preparation method of a molybdenum disulfide nanotube comprises the following process steps:
1) paving 5g of molybdenum hexacarbonyl at the bottom of a ceramic crucible, placing a porous anodic aluminum oxide template with the aperture of 40nm above the molybdenum hexacarbonyl with an opening facing downwards, sealing the crucible, placing the crucible in a vacuum tube furnace, and introducing 10SCCM nitrogen to clean air in the furnace tube. Under the protection of 10SCCM nitrogen, heating to 100 ℃ and preserving heat for 60min, then continuing heating to 300 ℃ and preserving heat for 40min to obtain metal molybdenum deposition, and stopping heating;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with sulfur powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating to 200 ℃ under the protection of 10SCCM nitrogen, keeping the temperature for 60min, continuing heating to 650 ℃ and keeping the temperature for 100min, and stopping heating;
3) and (3) when the temperature of the ceramic crucible in the step 2) is reduced to room temperature, taking out the sample, removing the porous alumina template by using a phosphoric acid solution with the concentration of 3mol/L, removing redundant sulfur powder by using carbon disulfide, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain a finished product of the molybdenum disulfide nanotube powder material in the embodiment 7.
Example 8
The finished products of the molybdenum disulfide nanotube powder materials prepared in the embodiments 1-7 are observed by a scanning electron microscope respectively, and the finished products are observed to form one-dimensional tubular structures with uniform tube wall appearance and uniform diameter, and have good crystallinity and strong controllability of nanotube appearance.
The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the scope of the present invention.
Claims (4)
1. A preparation method of a molybdenum disulfide nanotube is characterized by comprising the following process steps:
1) taking molybdenum hexacarbonyl as a raw material and porous anodic aluminum oxide as a template, paving the raw material at the bottom of a ceramic crucible, then placing a porous anodic aluminum oxide template with an opening downward above the raw material, sealing the crucible, placing the crucible in a vacuum tube furnace, heating under the protection of gas, sublimating at low temperature to deposit the molybdenum hexacarbonyl in the porous anodic aluminum oxide template, continuously heating to thermally decompose the molybdenum hexacarbonyl deposited in the porous anodic aluminum oxide template to obtain metal molybdenum deposit;
2) after the vacuum tube furnace in the step 1) is cooled to room temperature, taking out the porous anodic alumina template, placing the porous anodic alumina template into a ceramic crucible filled with sulfur powder with an opening facing downwards, sealing the crucible, placing the crucible into the vacuum tube furnace, heating under the protection of gas to enable elemental sulfur to directly react with metal molybdenum, stopping heating after the reaction is finished, and cooling the crucible to the room temperature along with the furnace;
3) removing the porous alumina template by using a dilute acid solution, removing redundant sulfur by using carbon disulfide, cleaning by using deionized water, then carrying out suction filtration treatment, and drying to obtain a finished product;
the low-temperature sublimation in the step 1) is carried out at the temperature of 50-150 ℃ for 30-200 min; the thermal decomposition temperature in the step 1) is 200-420 ℃, and the thermal decomposition time is 30-100 min; in the step 2), the reaction temperature of the elemental sulfur and the metal molybdenum is 500-650 ℃, and the reaction time is 100-150 min.
2. The method for preparing the molybdenum disulfide nanotube according to claim 1, wherein: the aperture of the porous anodic alumina template in the step 1) is within the range of 10-200 nm.
3. The method for preparing the molybdenum disulfide nanotube according to claim 1, wherein: the diluted acid solution in the step 3) is a phosphoric acid solution with the concentration of 0.1-3 mol/L.
4. The method for preparing the molybdenum disulfide nanotube according to claim 1, wherein: in the step 1) and the step 2), the gas is nitrogen or argon, the gas purity is 99.999%, and the flow rate of the protective gas is 10-500 SCCM.
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